反应详情

Step 78e) To a mixture of the acid (0.33 g, 0.71 mmol) of the product of Step 78d (Example 78), diisopropylethylamine (0.5 mL, 3.6 mmol), TFA salt (0.205 g, 0.51 mmol) of 1-Cyclopropylmethyl-cyclopropanesulfonic acid (1-amino-2-vinyl-cyclopropanecarbonyl)-amide, and HOBt (0.1 g, 0.6 mmol) in CH2Cl2 (8 mL) was added HATU (0.35 g, 0.92 mmol). The reaction mixture was stirred at rt overnite and diluted with EtOAc, washed with pH 4.0 buffer, dried (MgSO4), removed the solvent in vacuo. The residue was purified by PTLC to provide the product in 59% (0.22 g) yield: 1H NMR (methanol-d4) □ ppm 0.64 (m, 1H), 0.96 (m, 2H), 1.33 (m, 8H), 1.39 (m, 9H), 1.90 (m, 2H), 2.18 (m, 1H), 2.54 (m, 1H), 2.81 (m, 1H), 4.01 (m, 5H), 4.44 (d, J=28.99 Hz, 1H), 5.08 (m, 1H), 5.31 (m, 1H), 5.57 (s, 1H), 6.03 (m, 1H), 6.94 (s, t H), 7.27 (d, J=8.24 Hz, 1H), 7.64 (m, 1H), 7.92 (m, 1H), 8.14 (m, 2H), 8.66 (s, 1H), 8.74 (s, 1H).

1. washwashed with pH 4.0 buffer
2. dry with materialdried (MgSO4)
3. customremoved the solvent in vacuo
4. customThe residue was purified by PTLC
5. customto provide the product in 59% (0.22 g) yield